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In this work a comparative study of Screen‐Printed Carbon Electrodes (SPCE) – bare and modified by drop casting with carbonaceous nanomaterials (CNMs) as Multi Walled Carbon Nanotubes (MWCNT), Carbon Black and Functionalized Carbon Black for voltammetric determination of 5‐methyl‐6‐nitro‐7‐oxo‐4,7‐dihydro‐1,2,4‐triazolo[1,5‐a]pyrimidinide l‐arginine monohydrate (Triazid) as a potential drug with a broad spectrum of antiviral activity is reported. Bare SPCE and CNMs modified SPCE (SPCE/CNMs) have been characterized morphologically by SEM and electrochemically by cyclic voltammetry/electrochemical impedance spectroscopy with [Fe(CN)6]4−/3− as redox probe. Significant improvement of electrochemical performances is achieved with SPCE/CNMs compared with the bare SPCE. Among SPCE/CNMs studied SPCE modified with MWCNT (SPCE/CNT) is characterized by the best combination of electrochemical properties and electroanalytical performance towards TD. The linear dynamic range is 25–200 mg L−1 (R2=0.9975) with the limit of detection – 2.8 mg L−1 Triazid using SPCE/CNT and Square‐Wave Voltammetry technique. The developed sensor was successfully used for Triazid determination in the Pharmaceutical Substance "TRIAZID". The results achieved with SPCE/CNMs after chemical binding of dissolved oxygen in 0.04 M Britton‐Robinson buffer+0.04 M Na2SO3 (pH 7.2±0.2) are very useful for further development of cost‐effective and time‐consuming pharmaceutical routine assay. [ABSTRACT FROM AUTHOR]